CN100478687C - Evaluation method for raw material for magnet - Google Patents
Evaluation method for raw material for magnet Download PDFInfo
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- CN100478687C CN100478687C CNB2005100511775A CN200510051177A CN100478687C CN 100478687 C CN100478687 C CN 100478687C CN B2005100511775 A CNB2005100511775 A CN B2005100511775A CN 200510051177 A CN200510051177 A CN 200510051177A CN 100478687 C CN100478687 C CN 100478687C
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- 239000002994 raw material Substances 0.000 title claims description 17
- 238000011156 evaluation Methods 0.000 title claims description 15
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 110
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- 238000000034 method Methods 0.000 claims abstract description 69
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- 230000033228 biological regulation Effects 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052758 niobium Inorganic materials 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 4
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0579—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B with exchange spin coupling between hard and soft nanophases, e.g. nanocomposite spring magnets
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/03—Amorphous or microcrystalline structure
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/058—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IVa elements, e.g. Gd2Fe14C
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Mechanical Engineering (AREA)
- Power Engineering (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Continuous Casting (AREA)
Abstract
The invention relates to a method of evaluating a raw alloy for a magnet includes the steps of: measuring the quantity of heat that has been generated by a solidified alloy, which was obtained by rapidly cooling a melt of a magnetic alloy, during its crystallization; and estimating the percentage of an amorphous phase to the solidified alloy based on the heat quantity measured.
Description
Original bill application number: 01812176.4 (PCT/JP01/08317) the original bill applying date: September 25 calendar year 2001
Original bill denomination of invention: the manufacture method of using the raw alloy for nanocomposite type permanent magnet of thin strip casting method
Technical field
The present invention relates to employed permanent magnet such as various motors, instrument, sensor and loudspeaker raw alloy and manufacturing and evaluation method, in particular to raw alloy for nanocomposite type permanent magnet and the manufacturing and the evaluation method of making of the thin strip casting method.
Background technology
As the R-Fe-B series magnet, having developed institutional framework at present is R
2Fe
14Hard magnetics such as B phase and Fe
3Soft magnetisms such as B and α-Fe are (high magnetization ferromagnetism phase) nanocomposite type permanent magnet of combining mutually.By with resin material with nanocomposite type permanent magnet powder curing established practice setting shape, be made into isotropic bonded magnet and be used.
When making Nanocomposite magnet,, contain the quench solidification alloy of more noncrystalline tissue or noncrystalline phase in many using-systems as starting material.This quench solidification alloy carries out crystallization by thermal treatment, becomes finally that to have the average crystallite particle diameter be 10
-9M～10
-6The magnetic material of the micro organization about m.
The institutional framework of the magnetic alloy after the crystallization thermal treatment depends on the preceding quench solidification alloy organizing structure of crystallization thermal treatment to a great extent.Therefore, how to select to determine the chilling condition etc. of the alloy liquation of quench solidification alloy microstructure (ratio of noncrystalline phase etc.), have for manufacturing excellent magnetic property Nanocomposite magnet be very important.
At present, as the above-mentioned method for making that contains the quench solidification alloy of more noncrystalline phase like that, be the quick cooling method of well-known use device shown in Figure 1.In the method, the porose nozzle from the bottom, the rotation roller of making to copper etc. sprays molten alloy, by with the molten alloy chilling, makes the thin ribbon shaped solidified superalloy of noncrystallineization.
About said method, up to now, the research and the report of the university of existing research magnetic material, mechanism etc.But, employed device all only in nozzle with the equipment of the alloy fusion of tens of grams～hundreds of grams and the experimental size that sprays, with the little device of this treatment capacity, not can manufacture the Nanocomposite magnet raw alloy.
Increase the method for treatment capacity, for example open flat 2-179803 communique, spy and open flat 2-247305 communique, spy and open flat 2-247306 communique, spy and open flat 2-247307 communique, spy and open flat 2-247308 communique, spy and open flat 2-247309 communique, spy and open on the flat 2-247310 communique etc. on the books the spy.
In said method, with the alloy liquation that fuses in the calciner, injecting the bottom has in the container of nozzle, applies certain pressure by the liquation in container then, allows liquation from nozzle ejection (hereinafter referred to as " spray to cast method ").Pressurization so on one side, on one side liquation is sprayed by nozzle method, the liquation bar (liquation stream) with very fast flow velocity slightly is vertically near the topmost that rotates roller, sprays.Injected liquation is rotating roller formation liquid hole, surface (puddle), and the surface of contact of this liquid hole and roller is made the thin ribbon shaped quick cooling alloy by chilling.
In above-mentioned spray to cast method because the alloy liquation is shorter with the contact length of rotation roller, therefore on the rotation roller not chilling be over, awing be cooled from the alloy that is in the condition of high temperature (as 700 ℃～900 ℃) after the rotation roller is peeled off.In the spray to cast method,, realize noncrystallineization of various alloys by carrying out such process for cooling.
But in the spray to cast method, if allow treatment capacity be increased to suitable suitability for industrialized production (according to appointment more than the 1.5kg/min), then along with the increase of liquation quantity delivered (liquation jet velocity), the consumption of nozzle is very big.This will cause, and the liquation quantity delivered changes in processing procedure, thereby can not keep stable quenched condition.And, also exist the too high problem of expense that spends on the nozzle.In addition, because the bore of nozzle has restricted the jet velocity of liquation, therefore also exist the problem that is difficult to increase treatment capacity.
In addition, in the spray to cast method, also may produce because liquation solidifies in nozzle and causes the liquation phenomenon of blocking.Therefore be necessary to be provided with a mechanism that makes the container of being with nozzle remain on set point of temperature.For the emitted dose of maintenance liquation is certain, also be necessary to be provided with the upper surface of a control container inner melt and the mechanism of nozzle outlet pressure.Like this, just produced initial investment and the high problem of equipment operation cost that spends on the device.
And in the spray to cast method,, need make the jet velocity of liquation lower (below 1.5kg/min) for realizing the cooling velocity of stable obtained amorphous alloy, make production efficiency lower like this.In the spray to cast method, if the jet velocity of liquation is too high, just can not form the liquid hole on the roller surface, liquation is splashed.The result causes liquation cooling velocity instability.
In addition, the spray to cast method is to spray a spot of liquation by the roller to higher speed (as peripheral speed 20m/ more than second) rotation, makes to contain more amorphous quick cooling alloy.Therefore, the thickness of the thin ribbon shaped quick cooling alloy of making is typically below 50 μ m.This very thin thin ribbon shaped alloy is difficult to carry out effective recovery of high volume density.
On the other hand, as the method for making quick cooling alloy, known thin strip casting method in addition.In the thin strip casting method, supply with the alloy liquation from calciner to groove (tundish), by allowing the alloy liquation on the groove contact the making quick cooling alloy with chill roll.Groove is to store liquation and the flow velocity of control liquation and liquation stream carried out rectification, realizes stably supplying with continuously to chill roll the liquation guiding device of liquation thus for temporary transient.With the liquation that the chill roll external peripheral surface contacts, the chill roll that is rotated pulls, and moves along the roller periphery, is cooled in this process.
In the thin strip casting method, because the contact length of the liquation of roller circumferencial direction and roller outer circumference surface is longer, the cooling of liquation has just been finished on roller substantially.
As mentioned above, in the thin strip casting method, do not use the such jet blower of spray to cast method, but provide the alloy liquation continuously to the rotation roller, therefore be fit to produce in enormous quantities, manufacturing cost is descended by groove.
But, in the thin strip casting method,, chilling speed is reduced owing to the alloy liquation that provides to roller is more, this is unfavorable to the solidified superalloy of making noncrystallineization.Under the slow situation of chilling, easily make the alloy of noncrystalline mutually less (being that crystalline structure is more).In alloy structure, if there is more crystalline structure, then when follow-up crystallization thermal treatment, the part that has become crystallization makes crystalline structure become thick as nuclear.Therefore can not obtain having the Nanocomposite magnet of excellent magnetic property.
Therefore, the thin strip casting fado be used to make complete crystallization the metal Cast Strip (as, the spy opens flat 8-229641 communique).The quick cooling alloy of making like this, being generally used for principal phase is R
2F
14The raw alloy that the sintered magnet of B phase is used, and can not be used for the raw alloy that Nanocomposite magnet is used.
It is just difficult like this, efficiently and at low cost to make that Nanocomposite magnet is used, as to contain more noncrystalline tissue raw alloy.
The present invention in view of the above problems, purpose provides the raw alloy that nano composite permanent magnet cheap, that have good magnetic characteristics is used.
Summary of the invention
The manufacture method of raw material for magnet of the present invention comprises:
Making Fe
100-x-y-zR
xQ
yM
z(R is the element more than a kind or 2 kinds among Pr, Nd, Dy or the Tb, Q is a kind or 2 kinds a element among B or the C, M is the element more than a kind or 2 kinds among Co, Al, Si, Ti, V, Cr, Mn, Ni, Cu, Ga, Zr, Nb, Mo, Ag, Pt, Au, the Pb, x in the formula, y, z are respectively 1 atom %≤x＜6 atom %, 15 atom %≤y≤30 atom %, 0 atom %≤z≤7 atom %) operation of the alloy liquation of expression; And
Under the condition of vacuum or decompression, use that above-mentioned alloy liquation contact with chill roll to make along the axis direction of above-mentioned chill roll and mode with regulation contact width, rotation by above-mentioned chill roll, make the outer circumference surface of the above-mentioned chill roll in above-mentioned alloy liquation one edge move the thin strip casting method of cooling off on one side, the operation of making the thin ribbon shaped alloy that contains noncrystalline tissue;
And above-mentioned chill roll is with 3m/ more than second, the not enough 20m/ peripheral speed rotation of second, is that feed speed below the above 5.2kg/min/cm of 0.2kg/min/cm is supplied with above-mentioned alloy liquation continuously to above-mentioned chill roll with the feed speed of unit contact width.
In preferred embodiment,, supply with above-mentioned alloy liquation to above-mentioned chill roll with the feed speed more than the above-mentioned 3kg/min.
In preferred embodiment, utilize the groove of may command towards at least a portion liquation stream of the alloy liquation of above-mentioned chill roll, above-mentioned alloy liquation is contacted with above-mentioned chill roll, above-mentioned groove is positioned near the above-mentioned chill roll, the liquation discharge portion that has a plurality of regulation fluid width along the axis direction of above-mentioned chill roll, thus, the above-mentioned alloy liquation that contacts with above-mentioned chill roll by above-mentioned a plurality of liquation discharge portions forms many thin ribbon shaped alloys.
In preferred embodiment, the contact width of afore mentioned rules is 0.5cm～10.0cm.
In preferred embodiment, above-mentioned thin ribbon shaped alloy has the metal structure by the noncrystalline organizational composition more than the 60 volume % in fact.
In preferred embodiment, comprise the above-mentioned thin ribbon shaped alloy of continuous crushing, with 1g/cm
3Above volume density reclaims the operation of the alloy that is broken.
Raw material for magnet of the present invention is the raw material for magnet made from above-mentioned any one manufacture method, before crystallization thermal treatment, and intrinsic coercive force H
CJBelow 10kA/m.
In preferred embodiment, the thickness of above-mentioned raw material for magnet is 70～250 μ m.
The evaluation method of raw material for magnet of the present invention comprises: the coercitive operation of measuring the solidified superalloy of making by chilling magnetic alloy liquation; Calculate the operation of noncrystalline ratio contained in the above-mentioned solidified superalloy according to the coercitive size of said determination.
The evaluation method of raw material for magnet of the present invention comprises: the operation of measuring the crystallization thermal value of the solidified superalloy of making by chilling magnetic alloy liquation; Calculate the operation of noncrystalline ratio contained in the above-mentioned solidified superalloy according to the crystallization thermal value of said determination.
The manufacture method of raw material for magnet of the present invention comprises: use above-mentioned any one evaluation method to calculate the operation of noncrystalline ratio contained in the above-mentioned solidified superalloy; To the noncrystalline ratio with above-mentioned reckoning is that the above-mentioned solidified superalloy that the condition more than the regulation ratio is made carries out the heat treated operation of crystallization.
Description of drawings
Fig. 1 is nozzle in the existing spray to cast method and the side view that rotates roller.
Fig. 2 is for making the one-piece construction sectional view of the device of quick cooling alloy with the thin strip casting legal system in the embodiment of the present invention.
Fig. 3 is the chill roll in the device shown in Figure 2 and the vertical view of groove.
Fig. 4 is the thermal analysis curve of the sample powder before the thermal treatment of making in an embodiment.
Fig. 5 is the B-H loop of the sample powder before the thermal treatment of making in an embodiment.
Fig. 6 is near the enlarged drawing of initial point of Fig. 5.
Embodiment
The inventor is cheap for manufacturing cost to obtain, after heat treatment the raw alloy for nanocomposite type permanent magnet of good magnetic characteristics is arranged is purpose, and the manufacture method of the quench solidification alloy that contains more noncrystalline phase is studied.If with existing spray to cast method, also can make the quick cooling alloy that contains more noncrystalline phase that is suitable as raw alloy for nanocomposite type permanent magnet, still, realize that batch process then can produce above-mentioned problems.The inventor has courageously adopted with the spray to cast method and has compared the difficult amorphous thin strip casting method that forms, and the method for making the solidified superalloy that contains more noncrystalline phase of the thin strip casting method is studied.
Result of study is found, by determining that composition formula is Fe
100-x-y-zR
xQ
yM
z(R is the element more than a kind or 2 kinds among Pr, Nd, Dy or the Tb, Q is a kind or 2 kinds a element among B or the C, M is the element more than a kind or 2 kinds among Co, Al, Si, Ti, V, Cr, Mn, Ni, Cu, Ga, Zr, Nb, Mo, Ag, Pt, Au, the Pb, x in the formula, y, z are respectively 1 atom %≤x＜6 atom %, 15 atom %≤y≤30 atom %, 0 atom %≤z≤7 atom %) Biao Shi compositing range, can obtain the liquation that noncrystalline formation can be high, and this liquation is carried out chilling with the thin strip casting method.
And the inventor has also carried out conscientious research to the chilling condition that improves noncrystalline phase ratio when with the thin strip casting method alloy liquation with above-mentioned specific composition being carried out chilling.
Result of study shows, if have the alloy liquation of above-mentioned specific composition, then according to the feed speed of unit contact width be below the above 5.2kg/min/cm of 0.2kg/min/cm feed speed, be the thin strip casting method that chill roll that 3m/ second, above 20m/ rotated below second is supplied with liquation continuously to peripheral speed, can produce noncrystalline tissue and account for the above permanent magnet powder raw alloy of 60 volume %.In addition, according to this method, can the above liquation treatment capacity of 3kg/min make quick cooling alloy.
In the present invention, suitable liquation feed speed scope is to determine with the feed speed of above-mentioned unit contact width.This is because in the thin strip casting method, and liquation is to contact with chill roll in the mode that the axis direction along chill roll has a regulation contact width, and the liquation feed speed of the cooling condition of liquation and above-mentioned unit contact width has very big relation.In addition, the feed speed of typical unit contact width is that (unit: kg/min) width divided by the discharge portion of groove (is the contact width of liquation for the feed speed of using the liquation of supplying with to the groove of guiding liquation; Unit: cm) represent.In addition, when the discharge portion of groove has when a plurality of, use the feed speed of the liquation of supplying with to groove to represent divided by the summation of each discharge portion width.
If the liquation feed speed of unit contact width is excessive, the cooling velocity of the liquation by chill roll descends, the result can not promote its noncrystallineization, has made the quick cooling alloy that contains than the multiple crystallization tissue, and can not obtain being applicable to the raw alloy of Nanocomposite magnet.In addition, if the liquation feed speed is too small, be difficult to make liquation to contact with chill roll with suitable state with the thin strip casting method.Therefore, in the present invention, the feed speed of unit contact width is set in below the above 5.2kg/min/cm of 0.2kg/min/cm.
In addition, as described later, when for example contacting with chill roll by liquation,, can realize the treatment capacity that about 3kg/min is above by feed speed being set at more than about 0.5kg/min/cm with the contact form of contact site that 3 about 2cm of contact width are set.
Like this, by to the chill roll that rotates with the peripheral speed of above-mentioned particular range, with the feed speed supply liquation of above-mentioned particular range, promptly use the thin strip casting method also can make the quick cooling alloy that contains more noncrystalline tissue in high productivity ground.Because the thin strip casting method is not used the nozzle of the such remarkable increase manufacturing cost of spray to cast method, therefore needn't spend the expense of nozzle, the stopping production that causes because of the spray nozzle clogging accident can not appear yet.
Then, by the quick cooling alloy that obtains is heat-treated (below be also referred to as crystallization thermal treatment) about 550 ℃～about 750 ℃ temperature province for making its crystallization, can be made into mutually or Fe by α-Fe
3The soft magnetism of a kind or 2 kinds formation in the Type B compound mutually and have a R
2Fe
14The texture of the compound of Type B crystal structure coexistence account for more than 90%, mean grain size is nanocomposite type permanent magnet 10nm～50nm, that have good magnetic characteristics.
Below, with reference to accompanying drawing embodiment of the present invention is described.
Figure 2 shows that relevant with the embodiment of the present invention quenching apparatus 1 of making quick cooling alloy with the thin strip casting legal system.Quenching apparatus 1 have can make its inside be vacuum state or inert gas atmosphere decompression state main chamber 10 with by door to be opened/closed 28 ancillary chambers 30 that are connected with this main chamber 10.
10 inside is provided with in the main chamber: the calciner 12 that the fusion alloy raw material is used; Be used to make alloy liquation 3 chillings of supplying with by calciner, the chill roll 14 that solidifies; From the groove as liquation guiding device (tundish) 16 of calciner 12 to chill roll 14 guiding liquations 3; Be used to reclaim the retracting device 20 that solidifies the thin ribbon shaped alloy of peeling off from chill roll 14 back.
The liquation 3 that calciner 12 can be made the fusion alloy raw material is supplied to groove 16 with more stable quantity delivered.This quantity delivered can be by the adjustings arbitrarily such as tilting action of control calciner 12.
The periphery of chill roll 14 is to be made by the good material of heat conductivities such as copper, and diameter is 30cm～100cm, and width is 15cm～100cm.Chill roll 14 can rotate with predetermined rotational speed by not shown drive unit.By controlling this rotational speed, can regulate the peripheral speed of chill roll 14 arbitrarily.The cooling velocity of quenching apparatus 1 can be passed through the rotational speed of selection chill roll 14 etc., is controlled at about 10
2K/sec～about 2 * 10
4In the scope of K/sec.
The end 16a of groove 16 is arranged on and the line at top that links chill roll 14 and roller center at an angle on the position of θ.Be supplied to the liquation 3 of groove 16, be supplied to chill roll 14 by deadweight from end 16a.
By using groove 16, in the roll body direction (axis direction) of chill roll 14, can be on certain width, thickness supplies with liquation 3 with the broadening state equably.Groove 16 also has the function of the temperature of regulating the liquation 3 that will arrive chill roll 14 except that above-mentioned functions.The temperature of the liquation 3 on the groove 16 should be than more than the high 100K of liquidus temperature.This be because, if the temperature of liquation 3 is low excessively, have the primary crystal of baneful influence to give birth to nuclear in the part to the alloy characteristic behind the chilling, still residual after solidifying.Liquation retention temperature on the groove 16 can be controlled to the groove 16 cast melt temperature and the thermal capacity of groove 16 itself etc. constantly by regulating from calciner 12, and the firing equipment (not shown) of groove can be set as required.
Figure 3 shows that the groove 16 of present embodiment.The groove 16 of present embodiment at the relative end 16a that is provided with to ground with the outer peripheral face of chill roll 14, has a plurality of discharge portion 16b that are provided with predetermined distance distance W 2.The width of this discharge portion 16b (fluid width) W1 is preferably set to 0.5cm～10.0cm, more preferably 1.5cm～4.0cm.In the present embodiment, fluid width W 1 is set at 2cm.Be supplied to the liquation 3 of groove 16, with the axis direction A along chill roll 14 have with W1 be close to identical width state, contact with chill roll 14.Then, the liquation 3 so that fluid width W 1 contacts with chill roll 14 along with the rotation (roller 14 that is cooled is rolled) of chill roll 14 is moved on the roller periphery, is cooled in moving process.In addition, leak for preventing liquation, the distance between the end 16a of groove 16 and the chill roll 14 preferably sets below 3mm.
Gap W2 between adjacent discharge portion is preferably set to 1cm～10cm.If like this liquation contact site on the outer peripheral face of chill roll 14 (liquation cooling end) is divided into many places, then can cool off the liquation of discharging effectively from each discharge portion 16b.As a result,, also can reach desired cooling velocity, make the quick cooling alloy that contains the above noncrystalline tissue of 60 volume % even when increasing liquation quantity delivered to groove 16.Thus, can improve treatment capacity, produce quenched alloy for nano-composite magnet in batches.
In addition, the form of groove 16 is not limited to above-mentioned form, and a discharge portion both can have been arranged, and also can design the fluid width bigger.
Refer again to Fig. 2.The alloy liquation 3 that solidifies on the outer peripheral face of chill roll 14 becomes thin ribbon shaped solidified superalloy 3a, peels off from chill roll 14.The solidified superalloy 3a that peels off carries out fragmentation and reclaims in retracting device 20.
Retracting device 20 has the rotating blade 22 of broken thin ribbon shaped solidified superalloy 3a.Rotating blade for example can be a plurality of blades of being made by stainless steel etc., is driven by not shown drive unit, rotates with the speed about 500～1000rpm.Thin ribbon shaped solidified superalloy 3a from chill roll 14 is peeled off is imported into rotating blade 22 by guiding parts 24.Because therefore the solidified superalloy 3a thicker (70 μ m～250 μ m) that uses the present embodiment of thin strip casting method to make compares with the thin solidified superalloy that obtains with the spray to cast method, uses rotating blade 22 fragmentations easily.
In addition, because thin ribbon shaped solidified superalloy 3a is thicker like that as mentioned above, the length and width size that is rotated the solidified superalloy 5 of blade 22 fragmentations compares near 1.Therefore, can be with in the solidified superalloy 5 income returnable 26 of higher volume density after with fragmentation.Solidified superalloy 5 should be at least with 1g/cm
3Volume density reclaim.Can improve the recovery efficiency of operation like this.
Store the returnable 26 of the broken solidified superalloy 5 of ormal weight,, be sent to ancillary chamber 30 by mode of movements such as travelling belt (not shown).At this moment, before door 28 is opened, should allow the inside of ancillary chamber 30 in advance, be in vacuum or with the state of inert gas decompression as main chamber 10.Like this, could keep still being in the main chamber 10 vacuum or decompression state.After returnable 26 is transported from main chamber 10, close door 28, to keep the sealing of main chamber 10.
Then, in ancillary chamber 30,, give returnable 26 these upper cover 32 by not shown device.Like this, open door 34 to be opened/closed, the broken alloy 5 that is sealed in the returnable 26 is transported to the outside.
Like this, because the thin strip casting method do not use the used such nozzle of spray to cast method, can not produce because of nozzle diameter restriction jet velocity, because of in nozzle, solidifying problems such as causing the liquation obstruction, thereby be fit to production in enormous quantities.In addition, owing to do not need the firing equipment of spray nozzle part and, therefore can reduce initial stage equipment investment or equipment operation cost for controlling the pressure control mechanism of the anterior pressure of liquation.
In addition, because in the spray to cast method, nozzle segment can not utilize again, so the higher nozzle of processing cost has to throw away after having made.And in the thin strip casting method, groove can use repeatedly, and the equipment operation cost is reduced.
In addition, in thin strip casting method of the present invention, because the rotational speed of roller is lower, and the liquid outlet quantity of alloy is also than spray to cast fado, so the thickness of strip is thicker, so easy recovery.
[limiting the reason of forming]
Rare earth element R is for embodying the necessary hard magnetic phase of permanent magnet characteristic R
2Fe
14The necessary element of B.R of the present invention comprises the element more than a kind or 2 kinds among Pr, Nd, Dy and the Tb.But in order to adjust noncrystalline generation energy and crystallized temperature, also available above-mentioned other rare earth elements are in addition replaced a part of above-mentioned element.If it is the ratio of components of R is lower than 1 atom %, and is then less to improving coercitive effect, therefore inadvisable.On the other hand, if the ratio of components of R is more than the 6 atom %, then can not generate hard magnetic phase R
2Fe
14B significantly descends coercive force.Therefore, the ratio of components x of R is preferably 1≤x＜6.
Q is a kind or 2 kinds the element of B (boron) or C (carbon).B is the soft magnetism phase Fe as the principal phase of nanocomposite type permanent magnet material
3Iron-based borides such as B and hard magnetic be R mutually
2Fe
14The necessary element of B.If the ratio of components y of B exceeds the scope of 15 atom %～30 atom %, then can not embody the characteristic of permanent magnet, so the ratio of components y of B is preferably 15 atom %≤y≤30 atom %.In addition, in this instructions, " Fe
3B " also comprise and Fe
3B is difficult to the Fe of difference
3.5B.
And if B is lower than 15 atom %, then the noncrystalline generation of liquation can descend, and when making quick cooling alloy with the thin strip casting legal system as in the present invention, just can not make noncrystalline fully formation mutually.Even this quench solidification alloy is carried out crystallization thermal treatment, also can not get having the metal structure of good magnet characteristic.In addition,, can not influence magnetic characteristic and metal structure, therefore allow with the B of C displacement below 50%.
Remaining component is Fe.Replace a part of Fe with Co, can improve the rectangularity of demagnetizing curve, and can improve maximum magnetic energy product (BH)
MaxIn addition, the element substitution part Fe more than a kind or 2 kinds with among Al, Si, V, Cr, Mn, Ni, Cu, Ga, Zr, Nb, Mo, Ag, Ta, W, Pt, Au, the Pb also can improve the permanent magnet characteristic.But, can obtain Co, Al, Si, V, Cr, Mn, Ni, Cu, Ga, Zr, Nb, Mo, Ag, Ta, W, the Pt of above-mentioned effect, the total replacement amount z of the element more than a kind or 2 kinds among Au, the Pb, if surpass 7 atom %, can cause magnetization to reduce, so preferable range is 0≤z≤7 atom %.When replacement amount z when 0.5 atom % is above, can obtain more significant effect, therefore more preferably scope is 0.5 atom %≤z≤7 atom %.
[reason that qualification is created conditions]
In the present invention, use quenching apparatus 1 shown in Figure 2, the alloy liquation that will have above-mentioned specific composition carries out chilling, solidifies by the thin strip casting method, makes the thin ribbon shaped alloy.Under vacuum or the condition that reduces pressure with inert gas atmosphere, with the feed speed of unit contact width is feed speed below the above 5.2kg/min/cm of 0.2kg/min/cm, and the alloy liquation is supplied to chill roll with 3m/ peripheral speed rotation of not enough 20m/ second more than second.Like this, just can be made into quick cooling alloy with the above noncrystalline tissue of 60 volume %.Have at high proportion to this that the raw alloy of noncrystalline tissue carries out crystallization thermal treatment, just can be made into the nano combined property magnet that has excellent magnetic characteristics.
As mentioned above, with the peripheral speed of chill roll be set in 3m/ more than second the reason of not enough 20m/ second be: if the peripheral speed of roller is less than 3m/ second, then can be owing to the not enough quick cooling alloy that can not get containing noncrystalline tissue more than the 60 volume % of cooling power; If 20m/ more than second, then is difficult to roller liquation be rolled, cooled alloy is dispersed with laminar, reclaim very difficult.Best peripheral speed, because of the feed speed of the structure of chill roll, material, liquation etc. different.But if peripheral speed is too fast, resulting thin ribbon shaped alloy can be extremely thin, makes volume bulk, intractable.If peripheral speed is slow excessively, then be difficult to obtain sufficient cooling velocity, corresponding therewith, have to reduce the feed speed of liquation for improving cooling velocity, will cause production efficiency to reduce like this, reduced the benefit of using the thin strip casting method.Therefore, the peripheral speed of chill roll is preferably second 5m/ second～15m/.Second 6m/ second～10m/ more preferably.
As mentioned above, the reason that the feed speed of unit contact width is set in below the 5.2kg/min/cm is: if surpass 5.2kg/min/cm, then can not get the cooling velocity stipulated, therefore also just can not produce and contain amorphous quick cooling alloy more than the 60 volume %.The proper range of the feed speed of unit contact width, different according to the peripheral speed of roller, the structure of roller etc., but be preferably below the 4.0kg/min/cm, more preferably below the 3.0kg/min/cm.
In addition, the reason that the feed speed of unit contact width is set in more than the 0.2kg/min/cm is: if less than 0.2kg/min/cm, then use the thin strip casting method can not be stably to the liquation of chill roll supply flow rate abundance.Because it is insufficient that roller contacts with liquation, on chill roll, just can not stably form the liquid hole.Therefore, the thin ribbon shaped quick cooling alloy just forms part, is inhomogeneous quenched condition.Like this, if quenched condition fluctuates, just can not stably obtain containing the amorphous nano combined quick cooling alloy of using of ormal weight.
And, the liquation processing speed that device is whole, if not enough 3kg/min, then production efficiency is low, and cheap raw material can not be provided, therefore preferably more than 3kg/min.In order to realize this high production efficiency, the condition of the feed speed that can be as mentioned above like that not only satisfy the unit contact width below the above 5.2kg/min/cm of 0.2kg/min/cm, but also the liquation that can handle more than the 3kg in 1 minute, it is very necessary then suitably selecting the shape of groove, chill roll and the peripheral speed of chill roll etc.
For example, as shown in Figure 3, using when having 3 width (fluid width) as the groove of the discharge portion 16b of 2cm, with the feed speed of 3.0kg/min when groove is supplied with liquation, because the liquation quantity delivered of unit contact width is: 3.0 (kg/min) ÷ (2 * 3) (cm)=0.5kg/min/cm, therefore can stably make the big quick cooling alloy of noncrystalline ratio.
In addition, when for example using the Cu system roller of the about 30cm～50cm of diameter, the about 50cm of width, if the peripheral speed of roller is second 5m/ second～10m/, the feed speed of unit contact width is preferably about 0.5kg/min/cm～3.0kg/min/cm.In this case, by using the groove of suitable shape, for example can carry out the chilling operation with the feed speed of 5kg/min～15kg/min.
In addition, the shape by suitable selection groove (tundish), the width of liquation discharge portion and radical, liquation feed speed etc., making the thickness of resulting thin ribbon shaped quick cooling alloy and width is very important in proper range.The width of thin ribbon shaped quick cooling alloy is preferably in 15mm～80mm scope.If the thickness of thin ribbon shaped alloy is thin excessively,,,, make the free face cooling insufficient, so inadvisable then because liquation is different with the cooling velocity of free face (molten surface) at the surface of contact of roller if blocked up because low can causing of volume density reclaimed difficulty.Therefore, the thickness of thin ribbon shaped alloy is preferably 70 μ m～250 μ m, more preferably 100 μ m～200 μ m.
In that to use inert gas to make indoor when being in decompression state,, when the chill roll high speed rotating, will be involved in the inert gas around the roller, thereby make state of cooling instability if the inert gas air pressure during casting is too high.On the other hand, if air pressure is low excessively, the thin ribbon shaped alloy from roller is peeled off can not cool off fast by inert gas, therefore produces crystallization, contains noncrystalline many alloys thereby can not make.At this moment, the magnetic characteristic of the alloy that obtains after the crystallization thermal treatment is lower.Therefore, the pressure of inert gas preferably is adjusted into 1～50kPa.
[evaluation method of quick cooling alloy]
As mentioned above, with in the metal structure of thin strip casting manufactured if there is more crystalline structure, then when subsequent handling is heat-treated, original crystalline portion will become greatly, and magnetic characteristic is had adverse effect, this is undesirable.Thereby it is very important containing noncrystalline more alloy with the making of thin strip casting method, and for this reason, the amorphous ratio that can measure the actual quench solidification alloy of making quantitatively is favourable.
The inventor finds, by the thin ribbon shaped alloy fragmentation after will cast, and the thermal value when utilizing the heat analysis to try to achieve crystallization, just can be easy and the amount of the noncrystalline phase of quantitative evaluation accurately, thus used this method.
Shown in the embodiment of back, like that, can judge with this evaluation method, as principal phase Fe
3The thermal value of B phase through the heat treated magnet powder of the crystallization of back, has good magnetic characteristic when 28J/g is above.Because the thermal value of principal phase of 100% amorphous alloy of thinking with the making of too fast cooling velocity is measured as about 45J/g, therefore the implication of the above thermal value of the above-mentioned 28J/g of having is to become the alloy structure by noncrystalline organizational composition more than the 60 volume % in fact.
In addition, the inventor finds, by the fragmentation of the thin ribbon shaped alloy after will cast and measure its intrinsic coercive force, can be easy and the amorphous amount of quantitative evaluation accurately, thus used this method.
Because it is intrinsic coercitive that noncrystalline tissue is considered to almost not have, therefore, if the intrinsic coercive force H of the actual thin ribbon shaped quick cooling alloy of making
CJVery little, just can think and make the alloy that contains more noncrystalline phase.Particularly, if the intrinsic coercive force H of the alloy before the crystallization thermal treatment
CJBelow 10kA/m, have good magnetic characteristic through the heat treated magnet powder of the crystallization of back, therefore just can judge intrinsic coercive force H
CJShould be preferably below 10kA/m.
[embodiment and comparative example]
By the composition shown in the No.1～No.11 of following table 1 each raw material is mixed, cast by the casting condition shown in the table 1 with the thin strip casting method.Then, the alloy that makes is pulverized, screened the following powder 20g of 150 μ m, obtain estimating with alloy powder (sample powder).Use alloy powder with these evaluations, carry out heat and analyze and the magnetic characteristic evaluation.Heat is analyzed (measuring the crystallization thermal value) and is used DSC (differential scanning calorimeter), at 550 ℃～650 ℃ temperature ranges, programming rate is under 10 ℃/minute the condition, the powder of 40mg to be measured.VSM (Vibrating Sample magnetometer: vibration sample type magnetometer), apply under the 1.6MA/m of magnetic field in maximum, the 50mg powder is measured is used in the magnetic characteristic evaluation.
Table 1
Shown in the following table 2 each sample powder (sample) No.1～No.11, the principal phase (Fe before the thermal treatment that obtains by the heat analysis
3B compound phase) coercive force (kA/m) before crystallization thermal value (J/g) and the thermal treatment.In addition, table 2 has also shown magnetic characteristic (remanence Br, the intrinsic coercive force H of these sample powder at the permanent magnet powder that carries out under the heat treatment temperature shown in the table 2 obtaining after 30 minutes the thermal treatment
CJ, maximum energy product (BH)
Max).
Table 2
Figure 4 shows that the thermal analysis curve that obtains by the heat analysis of the sample that has excellent magnetic characteristics after the thermal treatment.In thermal analysis curve, can see the crystallization of 2 of crystallization kinds of phases heating peak value in temperature-rise period.Crystallization thermal value shown in the table 2 is calculated by asking the 1st peak area.As known from Table 2, sample No.1～No.8 that embodiment makes, the principal phase crystallization thermal value of trying to achieve by the heat analysis is all above 28J/g, so can judge that these samples are to be made of noncrystalline more than the 60 volume %.
Resulting B-H loop when being the sample of measuring after the thermal treatment that has excellent magnetic characteristics shown in Figure 5.Fig. 6 is near the enlarged drawing Fig. 5 initial point.Sample No.1～No.8 that embodiment makes, the coercive force of trying to achieve by the magnetic characteristic evaluation is all less than 10kA/m.In addition, these are considered to after the casting the above amorphous sample of 60 volume % is arranged, and resulting magnetic characteristic has good value after the crystallization thermal treatment.
On the other hand, the sample No.9～No.11 shown in the comparative example, the crystallization thermal value of principal phase is less, and intrinsic coercitive value is bigger.Can judge that the sample shown in these comparative examples has only below the 30 volume % mutually noncrystalline under the state after the casting.Sample No.9 because B content is less in forming, noncrystalline formations can be low, so in resulting quick cooling alloy noncrystalline phase exist ratio lower.In addition, sample No.10 and No.11, the feed speed of crossing low or liquation owing to the peripheral speed of roller is too high, can not obtain sufficient cooling velocity, and the therefore noncrystalline ratio that exists mutually is lower.These comparative example samples, even carry out crystallization thermal treatment, also (No.1～No.8) magnetic characteristic is low than embodiment sample.This is owing to have a more crystallization phase before the thermal treatment, and thermal treatment makes crystal grain become thick to cause.
From measurement result as can be seen, having the raw alloy of the permanent magnet powder of good magnetic characteristics after the thermal treatment, should major part be non-crystalline state.The present invention does not use the existing spray to cast method that is not suitable for producing in enormous quantities by adopting specific compositing range and creating conditions, but the low thin strip casting method of use cost, makes to contain noncrystalline raw alloy more than 60 volume %.
The possibility that industry is utilized
The invention provides the system of making the nano composite raw material for magnet with the thin strip casting legal system Making method. By in industrial production, adopting the method, compared with prior art, can be with low Cost make the nano composite raw material for magnet. Because the present invention has adopted production cost Low thin strip casting method be fit to be produced in enormous quantities, can provide cheap, have the hard iron oxygen magnet The permanent magnet powder of inaccessible excellent magnetic property.
Claims (2)
1. the evaluation method of a raw material for magnet is characterized in that: comprising:
Mensuration is by chilling Fe
100-x-y-zR
xQ
yM
zThe coercitive operation of the solidified superalloy that the alloy liquation of expression is made, wherein, R is the element more than a kind or 2 kinds among Pr, Nd, Dy or the Tb, Q is a kind or 2 kinds a element among B or the C, M is the element more than a kind or 2 kinds among Co, Al, Si, Ti, V, Cr, Mn, Ni, Cu, Ga, Zr, Nb, Mo, Ag, Pt, Au, the Pb, x in the formula, y, z are respectively 1 atom %≤x＜6 atom %, 15 atom %≤y≤30 atom %, 0 atom %≤z≤7 atom %;
Calculate the operation of noncrystalline ratio contained in the described solidified superalloy according to the coercitive size of described mensuration.
2. the manufacture method of a raw material for magnet is characterized in that: comprising:
Use the described evaluation method of claim 1 to calculate the operation of noncrystalline ratio contained in the described solidified superalloy;
To the noncrystalline ratio with described reckoning is that the described solidified superalloy that the condition more than the regulation ratio is made carries out the heat treated operation of crystallization.
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| CNB2005100511775A Expired - Fee Related CN100478687C (en) | 2000-10-06 | 2001-09-25 | Evaluation method for raw material for magnet |
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Also Published As
| Publication number | Publication date |
|---|---|
| EP1338359A4 (en) | 2006-06-07 |
| JPWO2002030595A1 (en) | 2004-02-19 |
| US7004228B2 (en) | 2006-02-28 |
| EP1338359B1 (en) | 2007-11-21 |
| US7547365B2 (en) | 2009-06-16 |
| CN1440317A (en) | 2003-09-03 |
| EP1880782A3 (en) | 2013-04-17 |
| EP1880782B1 (en) | 2015-01-07 |
| DE60131561T2 (en) | 2008-03-06 |
| AU2001288123A1 (en) | 2002-04-22 |
| CN1657936A (en) | 2005-08-24 |
| EP1338359A1 (en) | 2003-08-27 |
| WO2002030595A1 (en) | 2002-04-18 |
| CN1228158C (en) | 2005-11-23 |
| US20060081308A1 (en) | 2006-04-20 |
| EP1880782A2 (en) | 2008-01-23 |
| JP4787459B2 (en) | 2011-10-05 |
| DE60131561D1 (en) | 2008-01-03 |
| US20030183305A1 (en) | 2003-10-02 |
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